Sampling device and method of use thereof

ABSTRACT

An sampling device for capturing a material sample and a method of using said device to process said material sample in situ within the device. Embodiments of the invention may be disposed as elongate probes having extendable sample capture elements. A sample capture element of such a device may include a sample capture pocket located near a distal end thereof for capturing and trapping a sample of material. The sample capture pocket may be provided with a port for receiving material therein and a port for expelling material therefrom. These ports may be placed in communication with corresponding material transfer channels extending through the sample capture element to allow for the in situ processing of a material sample, and the subsequent discharge of the sample to an analyzer or another downstream location.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a continuation of U.S. application Ser. No.12/823,718, which was filed on Jun. 25, 2010, and is also a continuationof U.S. application Ser. No. 12/823,655, which was filed on Jun. 25,2010, both of which are hereby incorporated by reference.

TECHNICAL FIELD

The present invention is directed to material sampling devices and tomethods of using such sampling devices to capture material samples andto process material samples in situ.

BACKGROUND

As would be obvious to one of skill in the art, there are a number ofsituations and/or processes for which it would be desirable to extract asample of a material from a vessel in which the material is contained.Such extraction would generally be desirable for purposes of examinationor testing, but could be performed for other reasons, as well.

With respect to process monitoring, such sample extraction may bedesirable in a number of processes, including without limitation,parallel synthesis (combinatorial chemistry) applications, organicsynthesis, chemical process development, and the scale-up of laboratoryprocesses into production. A number of other such applications whereinsample extraction would be of interest also exist and would be known tothose of skill in the art.

Known sampling devices may be operated by hand, or may employ avacuum-based device mounted remotely or in a vessel containing amaterial of interest, or a by-pass port or similar mechanism throughwhich amount of a material of interest can be siphoned. In any case,however, known devices and methods generally require that an extractedsample be removed from the vessel and then transferred to anothercontainer before the sample can be quenched or similarly operated upon.

Known hand-operated devices commonly suffer from a lack of precisionwith regard to the timing of sample capture and subsequent samplemanipulation and, obviously, are typically not amenable to processautomation. Further, known hand-operated devices can only be operated totake samples that are at atmospheric pressure. Reactions that take placeunder pressure cannot be sampled with such hand operated devices. Aby-pass type of sampling device, where the reaction flows through a loopto a point where it can be sampled, can be used to sample reactionsunder pressure—however, a large reaction volume is required to use sucha device.

Known automated devices do not permit quenching, dilution, etc., to takeplace substantially contemporaneously with sample capture but, rather,require that a sample be first transferred to another vessel.Consequently, the state of a given sample may actually change from thetime of sample extraction to the time of quenching, etc.

Therefore, based on these foregoing issues with known sampling devices,it should be apparent that an in situ sampling device capable ofaccurately and repeatably capturing a material sample of known volumeand of quenching or otherwise processing a sample substantiallycontemporaneously with sample capture would be desirable. A samplecapture device of the present invention is such a device.

SUMMARY OF THE GENERAL INVENTIVE CONCEPT

Embodiments of the present invention may be disposed as elongate probeshaving extendable sample capture elements. Among other things, asampling device of the present invention may be used to sample smallreaction volumes (e.g., 5-100 μl), and to extract a sample from within areaction volume. Because a sampling device of the present invention is asealed unit, it can also be placed through a port into a pressurized orevacuated reaction chamber to sample a pressurized reaction volume. Asampling device of the present invention may also be used throughout awide temperature range (e.g., −40° C.-150° C.).

Unlike known devices, a sampling device of the present invention allowsfor substantially contemporaneous sample capture and sample processing(e.g., quenching, diluting mixing, etc.). Therefore, use of a samplingdevice of the present invention minimizes or eliminates any change insample conditions between the time of sample capture and sampleprocessing. This is not possible with devices currently known to theinventors.

In one exemplary embodiment, a sampling device of the present inventionmay include a substantially cylindrical and hollow outer tube of somelength. A proximal end of the outer tube may be clamped or otherwiseaffixed to a body portion of a probe actuator assembly. Concentricallyarranged within the outer tube at a distal end thereof is an assemblyincluding an outer sleeve, an inner sleeve and an extendable samplecapture element. A substantially frustoconical adapter is attached tothe distal end of the outer tube and tapers to a reduced diameter thatapproximates the diameter of the outer sleeve.

The outer sleeve is received in the adapter and retained therein byengagement between a collar of the outer sleeve and a shoulder in theadapter. A distal portion of the outer sleeve extends through thereduced diameter opening in the adapter and protrudes therefrom.

The inner sleeve includes a proximal portion having an inner and outerdiameter that is greater than the inner and outer diameter of a distalportion thereof. The distal and proximal portions of the inner sleeveare separated by a collar that forms a shoulder along both the interiorand exterior of the sleeve. The distal portion of the inner sleeveresides within the outer sleeve, with a bottom shoulder of the collarthereof in abutting contact with the collar of the outer sleeve. Thelarger diameter proximal portion of the inner sleeve extends into thedistal end of the outer tube.

Both the outer sleeve and the inner sleeve are held in position by theadapter, which presses an upper shoulder of the inner sleeve collartightly against the distal face of the outer tube when attached thereto.Consequently, when the adapter is fully assembled to the outer tube, theinner sleeve and the outer sleeve are held tightly together and are alsoprevented from movement with respect to the outer tube and the adapter.

The sample capture element is located to reciprocate within the innersleeve. The outer diameter of the sample capture element is provided tobe close in dimension to the inner diameter of the inner sleeve, suchthat a tight but slidable fit is produced therebetween. When the samplecapture element is in a retracted (closed) position, the distal endthereof may be positioned substantially even with the distal ends of theinner porting sleeve and the outer sleeve. When the sample captureelement is in an extended (sampling) position, the distal end thereofmay protrude from the distal end of the outer sleeve. The sample captureelement is provided with a concave sample capture pocket that, duringsample capture element extension, is exposed to and captures an amountof a sample of interest.

A proximal portion of the sample capture element extends into theenlarged inner diameter of the proximal portion of the inner sleeve. Theproximal end of the sample capture element is received within the distalend of a substantially hollow inner tube that is concentrically arrangedwithin the outer tube. The outer diameter of the inner tube approximatesthe inner diameter of the proximal portion of the inner porting sleevesuch that a tight but slidable fit is produced therebetween. The samplecapture element is retained in the inner tube, such as by a pin.

In an exemplary automated (autosampling) embodiment of a device of thepresent invention, a proximal end of the inner tube extends through theproximal end of the outer tube and is connected to an actuator (e.g.,pneumatic cylinder) that provides the desired extension and retractionof the sample capture element. In an exemplary hand-actuated (manual)embodiment of a device of the present invention, the inner tube may besimilarly connected to a hand-operable lever mechanism orlinearly-driven plunger that provides the desired extension andretraction of the sample capture element when manually actuated by auser of the device.

During extension and retraction of the sample capture element, thesample capture element is guided by contact between its exterior and theinterior of distal portion of the inner porting sleeve, as well as bycontact between the exterior of the inner tube and the interior of theproximal portion of the inner porting sleeve. Proper linear movement ofthe sample capture element is thus ensured. Rotation of the samplecapture element during reciprocation may be prevented if desired.

The sample capture element is ported to allow for purging/venting and toallow for the in situ processing (mixing, dilution, quenching, etc.), ofmaterial samples while located in the sample capture pocket thereof.Particularly, the sample capture pocket is provided with a supply portand a purge/vent port, each of which is associated with a correspondingchannel that runs through the sample capture element and exits throughthe proximal end thereof. Sample lines (e.g., tubing) may be connectedto each of these supply and purge/vent channels to lead processingmaterials to the sample capture pocket and to allow for venting and formaterial to be purged from the sample capture pocket. Such tubing may berouted through the inner tube. The distal portion of the inner sleeve isprovided with porting slots that allow the ports in the sample capturepocket to communicate with the corresponding channels in the samplecapture element during a processing (e.g., mixing, dilution, quenching)or purge/vent cycle.

In another exemplary embodiment, the above-described design may bealtered to have a fewer number of individual components. Particularly,in this alternative embodiment, the inner and outer sleeves and theadapter of the previously described embodiment are combined into asingle element. This element forms an end cap that threads into thedistal end of an outer tube and acts as a reciprocation guide andprotective cover for the sample capture element. The end cap containsinterior channels or grooves that connect the ports of the samplecapture pocket of the sample capture element to the channels of thesample capture element.

During use of either of these embodiments, the distal end of the probeis typically immersed in or held near the surface of a material fromwhich a sample is to be extracted. At the desired time, the samplecapture element is extended into the material, whereby an amount of thematerial fills the sample capture pocket and remains therein as thesample capture element is subsequently retracted back into the closedposition. With the sample of material trapped in the sample capturepocket, the sample may be processed, such as by contacting the samplewith a quenching or diluting substance so as to halt an ongoing reactionor dilute the sample, prior to transferring the sample of material toanother device or vessel.

When a sample capture element of a sampling device of the presentinvention is extended into a reaction volume to capture a sample, thesample lines are typically empty, having been purged for example, with agas or with a liquid that is neutral to the reaction being sampled. Asshould be apparent, when the sample capture element extends into thereaction volume, any material inside the sample capture pocket will comeinto contact with the reaction materials.

The choice of purge material may vary depending on the reaction beingsampled. For example a gaseous purge material may not be ideal if thereaction volume is small and the reaction is under pressure, as thepurge gas may cause a fluctuation in the reaction pressure. Similarly,any fluid present in the sample capture pocket when the sample captureelement extends will quickly mix with the reaction materials. It mustalso be considered that remnants of any quench media could compromise areaction.

While the sample capture element is extended, the sample lines that werepreviously empty, may be filled with quench media. The flow path throughthe sampling device may include transfer ports and a by-pass groove inthe sample capture element to allow flow in the fluid circuit when thesample capture element is in an extended position.

In the case of the aforementioned exemplary embodiments, the portingslots of the inner sleeve (or combined element) align with the samplecapture element transfer ports as the sample capture element reachesfull extension, allowing flow through the bypass groove and channels andwithin the sample line circuit. Quench media may, therefore, beintroduced to the sample capture element and possibly placed underpressure while the sample capture element is still extended. In thismanner, quench media is available to immediately flow into the samplecapture pocket and mix with the captured material sample upon retractionof the sample capture element and alignment of the sample capture pocketports with the porting slots of the inner sleeve.

Therefore, unlike known devices and methods, a sampling device of thepresent invention allows sample processing to occur while the capturedsample is still in the sampling device. Further, by providing a waitingsupply of quench media or other material, sample processing can beinitiated immediately upon retraction of the sample capture element.This ensures that the captured sample is preserved in a condition thatis as close as possible to the condition of the sample volume from whichit was extracted.

BRIEF DESCRIPTION OF THE DRAWINGS

In addition to the features mentioned above, other aspects of thepresent invention will be readily apparent from the followingdescriptions of the drawings and exemplary embodiments, wherein likereference numerals across the several views refer to identical orequivalent features, and wherein:

FIG. 1 is an exploded view of a portion of one exemplary embodiment ofan autosampling device of the present invention;

FIG. 2 a is an enlarged view in partial transparency of a distal portionof the autosampling device of FIG. 1 with a sample capture elementthereof in a retracted (closed) position;

FIG. 2 b shows the distal portion of the autosampling device of FIG. 2 awith the sample capture element thereof in an extended (sampling)position;

FIG. 3 is an enlarged view of a distal end of an exemplary samplecapture element of the present invention, wherein a ported samplecapture pocket is visible;

FIG. 4 a is an enlarged cross-sectional view of the distal portion ofthe autosampling device of FIG. 1, wherein the sample capture elementthereof is in a retracted (closed) position and a first (collectionmode) liquid flow path is shown;

FIG. 4 b shows the distal portion of the autosampling device of FIG. 4 awith the sample capture element thereof in an extended (sampling)position and a second (bypass mode) liquid flow path is shown;

FIG. 5 depicts the sample capture device of FIGS. 1-4 b in a fullyassembled condition;

FIG. 6 a shows an assembled distal portion of an alternate exemplaryembodiment of an autosampling device of the present invention, with anassociated sample capture element thereof in a retracted (closed)position;

FIG. 6 b shows the autosampling device of FIG. 5 a with the samplecapture element thereof in an extended (sampling) position;

FIG. 7 is a cross-sectional view of the distal portion of theautosampling device shown in FIGS. 5 a-5 b;

FIG. 8 is an enlarged perspective view of an exemplary sample captureelement that may be used with the autosampling device of FIGS. 6 a-6 band FIG. 7;

FIG. 9 a is a transparent view depicting an alternate embodiment of asample capture element and associated sleeve of the present invention,with the sample capture element in an extended position;

FIG. 9 b is an enlarged view of a portion of the sample capture elementand sleeve of FIG. 9 a;

FIG. 10 a is a transparent view showing the sample capture element andassociated sleeve of FIG. 9 a in a retracted position;

FIG. 10 b is an enlarged view of a portion of the sample capture elementand sleeve of FIG. 10 a;

FIG. 11 is an isometric view of one exemplary embodiment of ahand-actuated (manual) sampling device of the present invention;

FIG. 12 is a front view of the manual sampling device of FIG. 11 withconnections therefrom to a material introduction device and a samplecollection vessel schematically represented;

FIG. 13 is a process diagram illustrating one exemplary method ofoperating an autosampling probe of the present invention; and

FIG. 14 is a process diagram illustrating one exemplary method ofoperating a manual sampling probe of the present invention.

DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENT(S)

One exemplary embodiment of a sampling device 5 of the present inventionis illustrated in FIGS. 1-5. In this case, the device is an autosamplingdevice 5, as explained in more detail below. However, such a design mayalso be substantially used in a hand-actuated (manual) version of asampling device according to the present invention. A partial inventoryof the components of this device 5 are illustrated in the exploded viewof FIG. 1.

As shown, this autosampling device 5 includes a substantiallycylindrical and hollow outer tube 10 of some desired length. A proximalend 10 a of the outer tube 10 may be clamped or otherwise affixed to abody portion 255 of a probe actuator assembly 250, as shown in FIG. 5. Adistal end 10 b of the outer tube 10 is threaded as shown. In this case,the threads 15 are externally disposed on the outer tube 10, althoughinternal threading may be provided in other embodiments. The outer tube10 may be constructed from various materials depending on the substancesto which it might be exposed. It has been found, however, that acorrosion resistant metal alloy such as a HASTELLOY alloy (e.g.,HASTELLOY C-22 or C-276), is particularly well-suited for this purpose.HASTELLOY alloys are available from Haynes International, Inc.

Concentrically arranged within a distal portion of the outer tube 10 isa sample capture assembly 20 that includes an outer sleeve 30, an innersleeve 40, an extendable sample capture element 60, and a clampingadapter 25.

The clamping adapter 25 of this particular autosampling device 5 issubstantially frustoconical in shape, with a proximal portion 25 a oflarger diameter than a distal portion 25 b thereof. The proximal end ofthe adapter 25 is internally threaded to engage the threaded distal end10 b of the outer tube 10. External threading may be provided in otherembodiments having an internally threaded outer tube. Preferably, butnot essentially, the adapter 25 of this autosampling device 5 isconstructed from the same material as the outer tube 10.

The outer sleeve 30 is constructed as a elongate hollow tube of somelength, with a collar 35 of enlarged diameter encircling its externalproximal end 30 a. The outer sleeve 30 is received in the adapter 25 andpositioned therein by contact of a lower shoulder formed by the collar35 of the outer sleeve 30 and a corresponding shoulder 27 formed in theadapter (see FIGS. 4 a-4 b). In this embodiment of the autosamplingdevice 5, a distal portion 30 b of the outer sleeve 30 extends throughthe reduced diameter opening in the adapter and protrudes therefrom bysome predetermined distance. Preferably, the inner diameter of thedistal portion 25 b of the adapter 25 and the outer diameter of theouter sleeve 30 portion that passes therethrough are of dimensions thatproduces a slip fit therebetween.

The outer sleeve 30 may be constructed from various materials dependingon the materials to which it might be exposed. In this particularembodiment, the outer sleeve 30 is constructed of stainless steel.

The inner sleeve 40 is also constructed as a elongate hollow tube ofsome length. The inner sleeve 40 includes a proximal portion 40 a havingan inner and outer diameter that is greater than the inner and outerdiameter of a distal portion 40 b thereof. The distal and proximalportions 40 a, 40 b of the inner sleeve 40 are separated by a collar 45that forms a lower exterior shoulder 50 and upper interior and exteriorshoulders 55, 57. The distal portion 40 b of the inner sleeve 40 isreceived and resides within the interior of the outer sleeve 30. Theouter diameter of the distal portion 40 b of the inner sleeve 40 and theinner diameter of the outer sleeve 30 are each of a dimension thatresults in a sealing fit therebetween.

As shown in FIGS. 4 a-4 b, the longitudinal position of the inner sleeve40 within the outer sleeve 30 is set by contact between the bottomshoulder 50 of the inner sleeve collar 45 and the proximal end 30 a andcollar 35 of the outer sleeve 30. Preferably, the length of the distalportion 40 b of the inner sleeve 40 is such that the distal ends of theinner sleeve and outer sleeve 30 are aligned when the inner sleeve isinstalled in the outer sleeve.

The inner sleeve 40 may be constructed from various materials dependingon the substances to which it might be exposed. In this particularembodiment, the inner sleeve 10 is constructed of apolytetrafluoroethylene (PTFE) material, such as a TEFLON materialavailable from DuPont. An advantage to using a material such as TEFLONis that it is inert to most chemicals and has a low coefficient offriction.

It has also been found that the natural elasticity of PTFE allows it tocreate a good seal between the outer sleeve 30 and a sample captureelement 60 of the autosampling device 5. More particularly, theelastic-plastic behavior of such a material allows normal tightmanufacturing tolerances to be applied. In this case, the bore of theinner sleeve 40 may be made smaller than the outer diameter of a samplecapture element 60 described in more detail below) that reciprocatestherein, yet when the two components are fitted together the TEFLONyields at the inside bore and burnishes (i.e., the local yieldingpolishes the internal surface of the inner sleeve) during installation.Preferably, the inner diameter of the sleeve 40 is selected to maintainthe external fibers in the elastic state (until higher temperatures arereached) so that the sleeve provides a compressive sealing force againstthe sample capture element, thereby sealing the passages and transferpassages from communicating with adjacent passages.

When the adapter 25 and the inner and outer sleeves 30, 40 are installedto the distal end 10 b of the outer tube 10, the larger diameterproximal portion 40 a of the inner sleeve 40 extends into the distal endof the outer tube 10. The outer diameter of the proximal portion 40 a ofthe inner sleeve 40 and the inner diameter of the outer tube 10 are eachof a dimension that preferably results in a sealing fit therebetween.

Both the outer sleeve 30 and the inner sleeve 40 are held in position bythe adapter 25, which presses the upper outer shoulder 57 of the innersleeve collar 45 tightly against the distal face of the outer tube 10when the adapter is threaded onto the outer tube. The adaptor 25 acts asa clamping means to retain the outer sleeve 30 and the inner sleeve 40and to seal the outer tube 10 with the collar 45 of the inner sleevecollar 40. Concurrently, the inner sleeve 40 and the outer sleeve 30 arealso held tightly together and are prevented from longitudinal (linear)movement with respect to the outer tube 10 and the adapter 25.

As mentioned above, the sample capture assembly 20 also includes asample capture element 60. The sample capture element 60 is located toreciprocate within the inner sleeve 40, as can be best understood byreference to FIGS. 2 a-2 b and 4 a-4 b. To that end, the outer diameterof the sample capture element 60 and the inner diameter of the distalportion 40 b of the inner sleeve 40 are of a dimension that produces asealing but guided slidable fit therebetween.

The length of the sample capture element 60 may vary depending on thelength of the outer tube 10 and/or other components of the autosamplingdevice 5. Preferably, the length of the sample capture element 60 is atleast sufficient such that the proximal end thereof resides in theinterior of the proximal portion 40 a of the inner sleeve 40, whetherthe sample capture element 60 is in an extended or retracted position.

When the sample capture element 60 is in a retracted (closed) position,as shown in FIGS. 2 a and 4 a, the distal end 60 b thereof is preferablypositioned substantially evenly with the distal ends of the inner sleeve40 and the outer sleeve 30. When the sample capture element 60 is in anextended (sampling) position, as shown in FIGS. 2 b and 4 b, the distalend 60 b thereof protrudes from the distal ends of the inner sleeve 40and the outer sleeve 30 by some predetermined distance.

As most clearly shown in FIG. 3, the sample capture element 60 isprovided with a concave sample capture pocket 65 that, during samplecapture element extension, is exposed to and captures an amount of asample in which the distal end of the autosampling device 5 is immersed.The sample capture pocket 65 may be provided in different sizes tocapture different sample volumes (aliquots).

The sample capture element 60 may be constructed from various materialsdepending on the substances to which it might be exposed. In thisparticular embodiment, the sample capture element 60 is constructed of aceramic material. Sample capture elements of embodiments of the presentinvention may be resistant to strong acids and strong caustics.

The sample capture element 60 is ported to allow for purging/venting andto allow for quenching of material samples located in the sample capturepocket 65 thereof. Particularly, the sample capture pocket 65 isprovided with a quench port 70 and a purge/vent port 75, each of whichis associated with a corresponding channel 80, 85 that runs through thesample capture element 60 and exits through the proximal end 60 athereof. The distal portion 40 b of the inner sleeve 40 is provided withporting slots 90 that allow the ports 70, 75 in the sample capturepocket 65 to communicate with the corresponding channels 80, 85 in thesample capture element 60 during a quenching or purge/vent cycle.

The sample capture element 60 may also be provided with a by-pass groove240 that is placed in fluid communication with transfer ports 80 b, 85 bof the channels 80, 85 in the sample capture element by the portingslots 90 in the inner sleeve 40 to permit circulation of a quench mediawhile the sample capture element is in an extended position. This allowssample lines and the channels 80, 85 in the sample capture element 60 tobe filled with recirculating quench media as illustrated in FIG. 4 b.Quench media may, therefore, be introduced to the sample capture element60 and possibly placed under pressure while the sample capture elementis in an extended position. In this manner, quench media is available toimmediately flow into the sample capture pocket 65 and mix with acaptured sample upon retraction of the sample capture element andalignment of the sample capture pocket ports 70, 75 with the portingslots 90 of the inner sleeve.

As shown in FIG. 5, tubing 95 or similar conduit may be connected toeach of the quench and purge/vent channels 80, 85 to lead quenchmaterials to the sample capture pocket 65, and to allow for venting andfor material to be purged from the sample capture pocket. When flexibleplastic tubing is used for this purpose, ends of the tubing 95 may bepre-formed with threads by techniques known to those of skill in theart, the threaded ends may be subsequently trimmed to provide a uniformface to the threaded tube end, and the threaded ends of the tubing maybe engaged with like threaded sections provided in the proximal ends ofthe channels 80, 85. Upon threading the tubing into the associatedchannels in the sample capture element, the threaded ends of the tubingbottom out on the pilot diameter of the channels, thereby producing aseal. Such tubing 95 may be routed through an inner tube 100 (describedin more detail below) of the autosampling device 5.

The proximal end 60 a of the sample capture element 60 extending intothe interior of the proximal portion 40 a of the inner sleeve 40 isreceived within the distal end 100 b of a substantially hollow innertube 100 that is concentrically arranged within the outer tube 10. Asbest shown in FIGS. 4 a-4 b, the outer diameter of the inner tube 100approximates the inner diameter of the proximal portion 40 a of theinner sleeve 40, such that a sealing but slidable fit is producedtherebetween.

In this embodiment, the proximal end 60 a of the sample capture element60 is retained in the distal end 100 b of the inner tube 100 by a pin105 that passes through corresponding holes in both components. As shownin FIG. 5, the proximal end 100 a of the inner tube 100 extends throughthe proximal end 10 a of the outer tube 10 and is connected to anactuator 260 that provides the desired extension and retraction of thesample capture element 60. Various types of actuators 260 may beemployed for this purpose and, therefore, the actuator is genericallyrepresented in FIG. 5. For example, and without limitation, the actuator260 but may be a powered linear actuator, such as a pneumatic cylinder.

Referring to FIG. 4 a, it can be observed that when the sample captureelement 60 is in a retracted position, a gap 110 exists between thedistal end 100 b of the inner tube 100 and the upper inner shoulder 55of the inner sleeve 40. The length of this gap 110 represents themaximum possible length of extension of the sample capture element 60because, as shown in FIG. 4 b, contact between the distal end 100 b ofthe inner tube 100 and the upper inner shoulder 55 of the inner sleeve40 will function as a hard stop with respect to sample capture element60 extension. Of course, the actuator 260 could also have a stroke thatis less than the gap 110 length, in which case contact between thedistal end 100 b of the inner tube 100 and the upper inner shoulder 55of the inner sleeve 40 may not occur.

During extension and retraction of the sample capture element 60, thesample capture element is guided by contact between its exterior surfaceand the interior surface of the distal portion 40 a of the inner sleeve40, as well as by contact between the exterior surface of the inner tube10 and the interior surface of the proximal portion 40 a of the innersleeve 40. Proper axial linear movement of the sample capture element 60is thus ensured.

It may be desirable to prevent rotation of the sample capture element 60such that repeated orientation of the sample capture pocket 65 duringsample capture element extension can be assured. As shown in FIGS. 4 a-4b, rotation of the sample capture element 60 of this embodiment of theautosampling device 5 is prevented by causing the ends of the innertube/sample capture element pin 105 to extend into linearly arrangedslots 115 in the proximal portion 40 a of the inner sleeve 40 (see FIG.1). Consequently, the sample capture element 60 is permitted toreciprocate along the longitudinal axis of the autosampling device 5,but is prevented from rotation with respect thereto.

During use of the autosampling device 5, at least the distal end of theprotruding outer sleeve 30 is typically immersed in a material fromwhich a sample is to be extracted. The depth of the material need onlybe sufficient to cover the extended portion of the sample captureelement. At the desired time, the actuator 260 is activated to extendthe sample capture element 60 as described above. This causes the samplecapture element 60 to enter the material to be sampled, whereby anamount of the material fills the sample capture pocket 65 and remainstherein as the actuator 260 is subsequently activated to retract thesample capture element back into its closed position.

With the sample of material trapped in the sample capture pocket, thesample may be quenched with a quenching media, as represented in FIG. 4a, so as to halt an ongoing reaction prior to transferring the sample ofmaterial to another device or vessel. The sample may also be dilutedbefore subsequent removal from the sample capture pocket. Suchoperational variations are described in more detail below.

Portions of another exemplary embodiment of a sampling device 150 of thepresent invention are depicted in FIGS. 6 a-8. This sampling device 150embodiment is similar to the autosampling device 5 described above, buthas a fewer number of individual components. Particularly, in thisalternative embodiment, the inner and outer sleeves 40, 30 and theadapter 25 of the previously described embodiment are combined into asingle end cap/sleeve 155 element (hereinafter “end cap” for brevity).

In this embodiment, a proximal portion 155 a of the end cap 155 isprovided with external threads 160 that engage internal threads 225 ofan outer tube 220. The proximal portion 155 a of the end cap 155 is oflesser diameter than a distal portion 155 b thereof, which results inthe formation of a shoulder 165 slightly distally of the end cap threads160. When the end cap 155 is threaded into the outer tube 220, theshoulder 160 is brought into contact with the distal end of the outertube 220 and the end cap is thus secured thereto. The proximal portion155 a of end cap 155 also extends into the interior of the outer tube220 and may produce sealing contact therewith.

The outer tube 220 may be constructed from various materials dependingon the substances to which it might be exposed. In this particularembodiment, the outer tube 220 is again constructed of a HASTELLOYmaterial in similar fashion to the outer tube 10 of the autosamplingdevice 5 of FIGS. 1-5.

The distal portion 155 b of the end cap 155 is provided with an axialbore 170, the diameter of which may approximate the outer diameter of asample capture element 175 that will pass therethrough. Consequently,the bore 170 acts as a reciprocation guide for the sample captureelement 175. The interior surface of the bore 170 also seals against theouter surface of the sample capture element 175.

To this end, while the end cap 155 may be constructed from variousmaterials depending on the materials to which it might be exposed, ithas been determined that the natural elasticity of PTFE creates a goodseal when used to construct the end cap. Particularly, it has been foundthat the natural elasticity of PTFE allows it to create a good seal withthe interior of the outer tube 220, as well as a good seal with theouter surface of the sample capture element 175 while still permittinglow-friction reciprocation of the sample capture element in the bore 170of the end cap 155.

When the end cap 155 is comprised of PTFE or a similar material, thebore therein may be made smaller than the outer diameter of a samplecapture element 175 so that when the two components are fitted togetherthe TEFLON yields at the inside bore and burnishes during installation.Preferably, the size of bore in the end cap 155 is selected to provide acompressive sealing force against the sample capture element 175.

For operations at higher temperatures, the end cap 155 may be fittedwithin a thin metal (e.g., HASTELLOY) sleeve. The sleeve operates tocontain expansion of the end cap 155 that results from highertemperatures, thereby maintaining the sealing capabilities of the endcap by balancing the expansive forces with the increased elasticity ofthe PTFE. This allows the sampling device 150 to be used and cycled atelevated temperatures while still maintaining proper function.

As with the previously described autosampling device 5, this samplingdevice 150 also includes a sample capture element 175. As described, andas best shown in FIG. 7, the sample capture element 175 is located toreciprocate within the bore 170 of the end cap 155. To that end, theouter diameter of the sample capture element 175 is close in dimensionto the inner diameter of the bore 170 in the end cap 155, such that atight but guided slidable fit is produced therebetween (as describedabove).

The length of the sample capture element 175 may vary depending on thelength of the outer tube 220 and/or other components of the samplingdevice 150. The length of the sample capture element 175 is at leastsufficient to extend beyond the proximal end 155 a of the end cap 155 bya distance that is minimally equivalent to the desired sample captureelement extension length.

As most clearly shown in FIGS. 7-8, the sample capture element 175 ofthis embodiment includes an elongate cylindrical body with an externallythreaded proximal end 175 a. As can be observed in FIG. 7, the threadedproximal end 175 a of the sample capture element 175 is received withina like-threaded distal end 230 b of a substantially hollow inner tube230 that is concentrically arranged within the outer tube 220. A collar180 of enlarged diameter may encircle the exterior of the sample captureelement 175 distally of the threads so as to abut the inner tube 230 andpermit secure threaded installation of the of the sample capture element175 thereto. As with the previously described autosampling device 5, theproximal end 230 a of the inner tube 230 extends through the proximalend 220 a of the outer tube 220 and may be connected in a similarfashion to an actuator (not shown) that provides the desired extensionand retraction of the sample capture element 175.

The sample capture element 175 of this embodiment may be constructed ofa HASTELLOY material, as described above, but may also be constructedfrom various other materials depending on the substances to which itmight be exposed and as long as the desired fit between cooperatingelements is preserved. For example, the sample capture element 175 mayalso be constructed of certain ceramic materials.

Referring to FIG. 7, it can be observed that when the sample captureelement 175 is in a retracted position, a gap 235 exists between thecollar 180 of the sample capture element 175 and the proximal end 155 aof the end cap 155. The length of this gap 235 again represents themaximum possible length of extension of the sample capture element 175because, as shown in FIG. 7, contact between the collar 180 and theproximal end 155 a of the end cap 155 will function as a hard stop withrespect to sample capture element 175 extension. An associated actuatorcould also have a stroke that is less than the gap 235, in which casecontact between the collar 180 and the proximal end 155 a of the end cap155 may not occur.

During extension and retraction of the sample capture element 175, thesample capture element is guided by contact between its exterior surfaceand the interior surface of the bore 170 in the end cap 155. Properaxial linear movement of the sample capture element 60 is thus ensured.Due to the secure threaded engagement of the sample capture element 175and the inner tube 230, rotation of the sample capture element 175 isprevented without interfering with the ability of the sample captureelement to reciprocate along the longitudinal axis of the samplingdevice 150.

When the sample capture element 175 is in a retracted (closed) position,as shown in FIGS. 6 a and 7, the distal end 175 b thereof is preferablypositioned substantially evenly with the distal end 155 b of the end cap155. When the sample capture element 175 is in an extended (sampling)position, as shown in FIG. 6 b, the distal end 175 b thereof protrudesfrom the distal end 155 b of the end cap 155 by some predetermineddistance.

As shown in FIGS. 6 a, 7 and 8, the sample capture element 175 is againprovided with a concave sample capture pocket 185 that operates asdescribed above to capture an amount of a sample in which the distal endof the sampling device 150 is immersed. The sample capture pocket 185may be provided in different sizes to capture different sample volumes.

The sample capture element 175 is again ported to allow forpurging/venting and to allow for quenching of material samples locatedin the sample capture pocket 185 thereof. To this end, the samplecapture pocket 185 is provided with a quench port 190 and a purge/ventport 195, each of which is associated with a corresponding channel 200,205 that runs through the sample capture element 175 and exits throughthe proximal end 175 a thereof. Porting grooves 210, 215 are provided inthe end cap 155 to allow the ports 190, 195 in the sample capture pocket185 to communicate with the corresponding channels 200, 205 in thesample capture element 175 during a quenching or purge/vent cycle.

As with the autosampling device 5 described above, a by-pass groove 240may be provided to permit circulation of a quench media while the samplecapture element 175 is in an extended position. Also in similar fashionto the autosampling device 5 described above, tubing or similar conduitmay be connected to each of the quench and purge/vent channels 200, 205to lead quench materials to the sample capture pocket 185, and to allowfor venting and for material to be purged from the sample capturepocket. Such tubing may again be routed through the inner tube 230 andmay be connected to the sample capture element 175 as previouslydescribed.

Use of the sampling device 150 occurs generally in the same mannerdescribed above with the respect to the autosampling device 5 of FIGS.1-5. That is, at least the distal end of the end cap 155 is typicallyimmersed in or suspended over a material from which a sample is to beextracted. At the desired time, the actuator (whether powered orhand-actuated) is activated to extend the sample capture element 175therefrom. This causes the sample capture element 175 to enter thematerial to be sampled, whereby an amount of the material fills thesample capture pocket 185 and remains therein as the actuator issubsequently activated to retract the sample capture element back intoits closed position.

With the sample of material trapped in the sample capture pocket 185,the sample may be processed such as for example, by mixing, by dilution,or by contacting with a quenching substance so as to halt an ongoingreaction prior to transferring the sample of material to another deviceor vessel. Such operational variations are described in more detailbelow.

An alternative exemplary embodiment of a sample capture element 300 andan associated sleeve element 345 are depicted in FIGS. 9 a-9 b and 10a-10 b. Such an embodiment may be effective when it is desired orrequired to construct a sample capture element from a hard material suchas a glass or a ceramic. Whereas small holes, channels and otherfeatures of a metallic sample capture element may be created by varioustechniques, including by EDM (electrical discharge machining)techniques, creating such small features in a glass, ceramic, etc.,sample capture element may be substantially more difficult, if notimpossible. Therefore, it has been found that with a sample captureelement made from such hard materials, moving the various passages(conduits) thereof to the outside surface allows the same function to beachieved while simplifying or permitting the necessary machining (orforming). Additionally, attachment of tubing or similar conduit may alsobe moved to the outside of the sample capture element, where there ismore space.

The exemplary embodiment of the sample capture element 300 is shown inan extended position in FIGS. 9 a-9 b and in a retracted position inFIGS. 10 a-10 b. Such sample capture element positions will bewell-understood by virtue of the previously described exemplaryembodiments of the present invention.

As shown, the sample capture element 300 again includes a concave samplecapture pocket 305 that, during sample capture element extension, isexposed to and captures an amount of a sample in which the distal end ofthe sample capture element 300 is immersed. The sample capture pocket305 may again be provided in different sizes to capture different samplevolumes (aliquots).

The sample capture pocket 305 is provided with a quench port 310 and apurge/vent port 315 that, when the sample capture element 300 is in aretracted position, are placed into fluid communication withcorresponding conduits 320, 325 that run longitudinally along theexterior surface of the sample capture element 300 and exit intoinlet/outlet ports 330, 335 near the proximal end 300 a thereof. Thisfluid communication is described in more detail below.

The sample capture element 300 may also be provided with a by-pass port340 that permits the supply and possible circulation of a quench mediathrough the conduits 320, 325 while the sample capture element is in anextended position. This quench media supply and/or recirculation isdescribed in more detail below.

The sample capture element 300 is shown to reside and reciprocate withina sleeve 345. As described above with respect to the previouslydescribed exemplary embodiments, the sleeve 345 may again bemanufactured from a PTFE material, such as TEFLON. The use of othersleeve materials may also be possible depending on the particularmaterial from which the sample capture element 300 is constructed. Theouter diameter of the sample capture element 300 and the inner diameterof the sleeve 345 are of a dimension that produces a sealing but guidedslidable fit therebetween, such that there is no leakage of fluid fromthe sample capture element conduits 320, 325.

As can be best observed in FIGS. 9 b and 10 b, the sleeve 345 isprovided with a pair of elongate and axially directed transfer ports 350that pass through the wall of the sleeve. As described in more detailbelow, the transfer ports 350 permit fluid communication between thesample capture element conduits 320, 325 and, depending on the positionof the sample capture element 300, either the sample capture elementby-pass port 340 or the quench port 310 and purge/vent port 315 in thesample capture pocket 305.

The sample capture element 300 is shown in an extended position in FIGS.9 a-9 b, wherein the sample capture pocket 305 is exposed for collectionof a sample from a material volume into which the sample capture pocketwould be immersed. As can be most clearly observed in FIG. 9 b, in thisposition, an arcuate section of each sample capture element conduit 320,325 is placed in fluid communication with a first end of the transferports 350 of the sleeve 345. Simultaneously therewith, the second end ofeach transfer port 350 is placed in fluid communication with the by-passport 340 in the sample capture element 300. Consequently, when thesample capture element 300 is in an extended position, a quench mediacan be supplied thereto and stored or allowed to recirculate through afluid path defined by the inlet/outlet ports 330, 335, the conduits 320,325, the transfer ports 350, and the by-pass port 340. Supplying quenchmedia to a sample capture element in this manner has already beengenerally explained above and, therefore, need not be restated here.

The sample capture element 300 is shown in a retracted position in FIGS.10 a-10 b, wherein the sample capture pocket 305 is withdrawn into thesleeve 345 to permit acting on a material sample trapped therein. As canbe most clearly observed in FIG. 10 b, when the sample capture element300 is in the retracted position, the arcuate section of each samplecapture element conduit 320, 325 is placed in fluid communication withthe second end of the sleeve transfer ports 350. Simultaneouslytherewith, the first ends of the transfer ports 350 are respectivelyplaced into fluid communication with the quench port 310 and purge/ventport 315 in the sample capture pocket 305. Consequently, when the samplecapture element 300 is in a retracted position, a sample in the samplecapture pocket 305 may be quenched, diluted, and removed therefrom toanother vessel or device, and the sample capture pocket may be purgedwith a gas or another fluid, via a fluid path defined by theinlet/outlet ports 330, 335, the conduits 320, 325, the transfer ports350, and the quench port 310 and purge/vent port 315. Operationalvariations are described in more detail below.

In any of the above-described exemplary embodiments of an samplingdevice of the present invention, the sampling device may be readied forsampling, such as by first cleaning the sampling lines (tubing) bypurging with neutral fluids, gases or an inert gas. It is also possibleto draw vacuum prior to purging of the sampling lines. Such cleaning maybe performed in a cyclic fashion to ensure that any impurities areremoved. Depending on the design of the sampling device, thequench/dilute lines can be pre-flooded with respective fluids.

At an appropriate time, the sample capture element is extended and analiquot of the reaction mixture is captured by the sample capturepocket. Depending on the material (e.g., the reaction mixture) beingsampled, the actual sampling can take place immediately after the samplecapture element is extended or with a certain time period thereafter,such that the sample capture pocket may be purged with the reactionmixture prior to taking a sample.

With a sample of material in the sample capture pocket, the samplecapture element is then retracted, trapping the sample of material inthe sample capture pocket and making it available for immediateprocessing. Depending on the scheme desired by a user of the samplingdevice, several actions can subsequently take place. First, the sampleof material may be contacted with a quench fluid, upon which thereaction is stopped very quickly, if not immediately. In this case, thesample of material represents the reaction mixture substantially as itexisted at the time of sampling. The quenched sample can then be dilutedand discharged to a respective analyzer, such as for example, a gaschromatograph, a HPLC, a combination of both, or one or more othersuitable analyzers. Under an alternative scheme, the sample may bediluted only, and discharged (e.g., forwarded to an analyzer) as iswithout first being quenched. Under yet another scheme, the sample isdiluted prior to being quenched. While this technique may be lessefficient, it may be necessary, for example, in a case where the quenchmaterial cannot be solved in the solvent used for the reaction. As aspecific example, it would be possible to take a sample from a biologicreaction and use a quench material that is only solvable in a toxicsolvent. The steps of quenching and dilution may also be combined inother ways not specifically described herein.

The steps of diluting and discharging a material sample may beaccomplished in various ways. For example, a continuous fluid (e.g., asuitable solvent or gas) stream may be used, which stream delivers thematerial sample to the analyzer. Alternatively, a specified amount ofdilution fluid may be cyclically pumped through a concentrated sampleand then used for sample discharge. In this technique, the sample willbe thoroughly mixed with the dilution fluid. Such a technique may bedesirable or necessary, for example, when sampling slurry reactionmixtures. It may also be possible to use a vacuum pump to cause thedischarging of a quenched, diluted or unaltered material sample.

An exemplary hand-actuated (manual) sampling device 400 of the presentinvention is illustrated in FIGS. 11-12. In a manner similar to that ofthe previously described sampling devices 5, 150, this manual samplingdevice 400 also includes a sample capture assembly 405 that includes anouter tube 410 within which is disposed a reciprocative sample captureelement 415. While the sample capture assembly 405 is shown herein to besimilar in construction to the sample capture assembly 20 of theexemplary embodiment shown in FIG. 1, it is to be understood that amanual sampling device of the present invention may also employ a samplecapture assembly of the design described with respect to the samplingdevice 150, or of a design not specifically shown and described herein.

This manual sampling device 400 also includes a body portion 420 thathouses a probe actuator assembly, of which only a lever 425 is visible.As indicated by the arrows, the lever 425 is rotatable between anextended position (as shown) and a position wherein the lever issubstantially pressed against the body portion 420 of the device 400. Inthis particular example, an inward movement of the lever 425 produces anextension of the shape capture element 415. Upon release of the lever425, a spring or similar mechanism retracts the shape capture element415 back into the outer tube 410 and returns the lever 425 to itsillustrated extended position. Such a mechanism should be well known toone of skill in the art and, therefore, is not described in furtherdetail herein.

In an alternate embodiment of a manual sampling device (not shown),reciprocation of the sample capture element may be accomplished by useractuation of a linear plunger assembly, such as one or more of theplunger assemblies commonly found on commercially available pipettesthat would be familiar to one of skill in the art.

The body portion 420 of this embodiment, as well as body portions ofother embodiments of a manual sampling device of the present invention,may be provided with a handle 430 or other features that facilitategrasping and/or manipulation by a user. The body portion of a manualsampling device of the present invention may also be shaped or contouredto facilitate grasping and/or manipulation by a user.

As shown, sampling lines 435 protrude from the manual sampling device400. As can be understood from the foregoing descriptions of othersampling device embodiments 5, 150, such sampling lines 435 are providedto supply processing materials (e.g., quench or dilution media) to thesample capture pocket of the sample capture element 415, and to carryaway materials purged from the sample capture pocket.

To this end, a supply sample line 435 a is depicted in FIG. 12 as beingconnected to a processing material supply device 440. In this particularexample, the processing material supply device 440 is shown to be amanually operable syringe that can be used to transfer quench, dilutionor other sample materials to the sample capture pocket of the device 400to process a material sample trapped therein. In other embodiments, thesyringe may be replaced with another manually operated device or with apowered and possibly automated device, such as a pump.

A purge sample line 435 b is depicted in FIG. 12 as being connected to avessel 445 for receiving material purged from the sample capture pocketof the sampling device 400. The vessel may simply be a container, or maybe a receptacle or other receiving element of an analyzer, such as oneof the analyzers described above.

While the structure of this manual sampling device 400 differs somewhatfrom the structure of the autosampling device 5 shown in FIG. 5, thefunction is still substantially the same. That is, the sample captureelement is still extended into a sample of interest at an appropriatetime and an aliquot of the sample is captured by the sample capturepocket. With a sample of material in the sample capture pocket, thesample capture element is then retracted, trapping the sample ofmaterial in the sample capture pocket and making it available forimmediate processing, as described above. Thus, the primary differencebetween an autosampling device and a manual sampling device of thepresent invention is simply the fact that the sample capture element ofan autosampling embodiment is extended/retracted by a powered actuator(e.g., a pneumatic cylinder), while the sample capture element of amanual sampling embodiment is extended/retracted by operator actuationof a manual actuator (e.g., a lever mechanism or linear plungerassembly).

One specific exemplary method of capturing, processing, and discharginga material sample using an autosampling device of the present inventionis diagrammatically illustrated in FIG. 13. In this particular example,a purge command is sent to the autosampling device 500 by a controllerin communication therewith. Once this purge command is received, thesampling lines of the autosampling device are purged with a suitablepurging material 405, such as a gas or neutral liquid retrieved from asource thereof. The status of the purging operation may be monitored510. In some cases, this purging step may be skipped during the processof acquiring a material sample.

Once the purging operation has been completed, or in cases where nopurging operation is practiced, a probe extend command may be sent 515to the autosampling device, which causes the sample capture element toextend from the outer tube and the sample capture pocket therein to beexposed to the material of interest 520, as has been described above.The state of sample capture element extension may be monitored 525 toensure that the sample pocket is fully exposed to the material to besampled.

In this particular example of autosampling device operation, thecaptured sample of material will be quenched. Consequently, once thesample capture element has been adequately extended, a capturepreparation command may be sent 530 to the autosampling device. In thisexample, this causes quench fluid to be pumped into the sampling lines535 of the autosampling device via the by-pass port in the samplecapture element. In other examples, wherein a by-pass port is notpresent, this quenching step may be delayed until after a materialsample has been captured and the sample capture element has beenretracted. The filling/circulation of the autosampling device samplinglines with quench fluid may be monitored 540 to ensure that quench fluidis available for mixing with a captured sample of material.

Once the quench fluid pumping operation is deemed acceptable, or incases where a quench fluid pumping operation is delayed (as describedabove) or where no the quench fluid pumping operation is practiced, asample capture command may be sent 545 to the autosampling device. Thiscauses the sample capture element of the autosampling device to retract550 into the outer tube, trapping a sample of material in the samplecapture pocket of the sample capture element and causing the materialsample to be quenched in situ by the quenching fluid residing in thesample capture element.

A selected acquisition command may subsequently be sent 555 to theautosampling device. This causes the material sample in the samplecapture pocket to be acquired (e.g., sent to an appropriateanalyzer(s)). In this particular example, acquisition may beaccomplished 560 by cyclically pumping a dilution fluid through thematerial in the sample capture pocket and then discharging the materialsample to its next destination, or by using a continuous fluid stream todilute and discharge the material sample to its next destination. Otherdilution/discharge methods and combinations of methods are alsopossible, as previously described herein.

The sample acquisition process may be monitored for completeness 565.Once sample acquisition is deemed to be complete, the operation mayreturn to the purging stage 500, or may await the next sample captureelement extension command if it is desired to skip the purging step orwhen no purging step is used.

An exemplary method of capturing, processing, and discharging a materialsample using the manual sampling device of FIGS. 11-12 isdiagrammatically illustrated in FIG. 14. In this particular example, thesampling lines of the manual sampling device may be purged 605 with asuitable purging material, such as a gas or neutral liquid, pumpedtherethrough by appropriate operation 600 of the syringe 440. In somecases, this purging step may be skipped during the process of acquiringa material sample.

Once the purging operation has been completed, or in cases where nopurging operation is practiced, the lever 425 of the sampling device 400is depressed, which causes the sample capture element to extend from theouter tube and the sample capture pocket therein to be exposed to thematerial of interest 620, as has been described above.

In this particular example of sampling device operation, the capturedsample of material will be quenched. Consequently, once the samplecapture element has been adequately extended, a syringe 440 is operated620 to transfer quench fluid under pressure into the sampling lines 635of the sampling device via the by-pass port in the sample captureelement. In other examples, wherein a by-pass port is not present, thisquenching step may be delayed until after a material sample has beencaptured and the sample capture element has been retracted.

Once the quench fluid transfer operation is deemed acceptable, or incases where a quench fluid transfer operation is delayed (as describedabove) or where no quench fluid transfer operation is practiced, thelever 425 of the sampling device 400 is released 630. This causes thesample capture element of the sampling device to retract 635 into theouter tube, trapping a sample of material in the sample capture pocketof the sample capture element and causing the material sample to bequenched in situ by the quenching fluid residing in the sample captureelement.

With the material sample trapped in the sample capture pocket, a syringe440 may be used to acquire the sample (e.g., to send the sample to anappropriate vessel, such as the vessel of an analyzer(s)). In thisparticular example, acquisition is accomplished by operating the syringe640 to push a dilution fluid through the sample lines and into thematerial in the sample capture pocket to discharge the material sampleto its next destination 645. In an alternate embodiment, a pump orsimilar device may be used to supply a continuous fluid stream to diluteand discharge the material sample to its next destination. Otherdilution/discharge methods and combinations of methods are alsopossible, as previously described herein.

With the current sample acquired 650, the operation may return to thepurging stage, or to the next sample capture element extension step ifit is desired to skip the purging step or when no purging step is used.

While certain embodiments of the present invention are described indetail above, the scope of the invention is not to be considered limitedby such disclosure, and modifications are possible without departingfrom the spirit of the invention as evidenced by the following claims:

What is claimed is:
 1. A sampling device for capturing a sample of amaterial of interest, said device comprising: a hollow outer tubeadapted for association with an actuator; a sample capture elementlocated within said hollow outer tube and reciprocatable by saidactuator; and a sample capture pocket in said sample capture element,said sample capture pocket located and shaped to capture a sample ofsaid material of interest upon extension of said sample capture elementfrom said hollow outer tube.
 2. The sampling device of claim 1, whereina proximal end of said hollow outer tube is secured to an actuatorassembly that includes said actuator.
 3. The sampling device of claim 1,wherein said sample capture pocket is shaped to repeatably capture aparticular volume of said material of interest.
 4. The sampling deviceof claim 1, wherein said sample capture pocket includes a port forreceiving material therein and a port for expelling material therefrom,said ports in communication with corresponding channels in said samplecapture element when said sample capture element is in a retractedposition.
 5. The sampling device of claim 4, wherein said channels insaid sample capture element are internal thereto.
 6. The sampling deviceof claim 4, wherein said channels in said sample capture element extendalong the external surface thereof.
 7. The sampling device of claim 4,further comprising a conduit connected to a proximal end of each channelin said sample capture element, said conduits for providing material tosaid sample capture pocket that is different from said capturedmaterial, and for transporting material from said sample capture pocket.8. The sampling device of claim 1, further comprising: a hollow clampingadapter securely affixed to a distal end of said outer tube; a hollowand cylindrical outer sleeve having a proximal end residing in saidclamping adapter and a distal portion that passes through a distalopening in said adapter to protrude therefrom; and a hollow andcylindrical inner sleeve, a distal portion of said inner sleeve residingin said distal portion of said outer sleeve and having a bore forreceiving said sample capture element, a proximal portion of said innersleeve extending into said distal end of said outer tube.
 9. Thesampling device of claim 8, wherein said sample capture element islocated partially within said distal portion of said inner sleeve, witha proximal end of said sample capture element extending into saidproximal portion of said inner sleeve.
 10. The sampling device of claim9, further comprising an inner tube arranged within said outer tube, aproximal end of said inner tube extending from said proximal end of saidouter tube and connected to said actuator, a distal end of said innertube connected to said proximal end of said sample capture element. 11.The sampling device of claim 1, wherein rotation of said sample captureelement is prohibited.
 12. A method of capturing a sample of a materialof interest, said method comprising: providing a sampling device, saidsampling device including a reciprocative sample capture element locatedwithin an outer tube and adapted for extension and retraction withrespect thereto; and a sample capture pocket located in said samplecapture element, said sample capture pocket adapted to capture a volumeof a material of interest via reciprocation of said sample captureelement; positioning a sampling end of said sampling device in or near asample of said material of interest; causing said sample capture elementof said sampling device to extend from said outer tube into saidmaterial of interest, thereby filling said sample capture pocket in saidsample capture element with an amount of said material of interest; andcausing said sample capture element of said sampling device to retractinto said outer tube, thereby trapping a sample of said material ofinterest in said sample capture pocket.
 13. The method of claim 12,wherein said sample capture pocket in said sample capture elementincludes a processing material receiving port and a material expulsionport therein; said ports are in communication with correspondingchannels in said sample capture element when said sample capture elementis in a retracted position; and sampling lines are associated with saidchannels in said sample capture element.
 14. The method of claim 13,further comprising purging said sampling lines and said sample capturepocket before extending said sample capture element into a material ofinterest.
 15. The method of claim 13, further comprising passing aquenching fluid through said sampling lines of said sampling devicewhile said sample capture element thereof is extended into a material ofinterest.
 16. The method of claim 13, further comprising: processingsaid sample of material in situ within said sample capture pocket; anddischarging said sample of material from said sample capture pocket to adownstream location.
 17. The method of claim 16, wherein the processingof said sample of material trapped in said sample capture pocketincludes quenching said sample by passing a quenching fluid thereto viasaid processing material receiving port.
 18. The method of claim 16,wherein the processing of said sample of material trapped in said samplecapture pocket includes diluting said sample by passing a dilutionmaterial thereto via said processing material receiving port.
 19. Themethod of claim 18, wherein a specified amount of dilution material iscyclically pumped through said sample of material prior to the dischargeof said sample of material by a dilution material.
 20. The method ofclaim 18, wherein a continuous flow of dilution material is used todilute and discharge said sample of material.
 21. The method of claim18, wherein said dilution material is selected from the group consistingof a gas, a liquid solvent, and a neutral liquid.
 22. The method ofclaim 16, wherein a sample of material is discharged to an analyzerselected from the group consisting of a gas chromatograph, a HPLCdevice, and a combination thereof.
 23. The method of claim 12, whereinsaid sampling device is an autosampling device, and wherein operatingcommands are sent to said autosampling device by a microprocessor-basedcontroller associated with another device used to control or analyze amaterial of interest.
 24. A method of performing in situ sample analysiscomprising: providing a sampling device, said sampling device includinga reciprocative sample capture element located within an outer tube andadapted for extension and retraction with respect thereto; and a samplecapture pocket located in said sample capture element, said samplecapture pocket adapted to capture a volume of a material of interest viareciprocation of said sample capture element; reciprocating said samplecapture element so as to contact and trap a sample of said material ofinterest in said sample capture pocket; processing said sample ofmaterial in situ within said sample capture pocket; and discharging saidsample of material from said sample capture pocket to a downstreamlocation.
 25. The method of claim 24, wherein the processing of saidsample of material trapped in said sample capture pocket includesquenching said sample by passing a quenching fluid thereto via aprocessing material receiving port in said sample capture pocket. 26.The method of claim 24, wherein the processing of said sample ofmaterial trapped in said sample capture pocket includes diluting saidsample by passing a dilution material thereto via a processing materialreceiving port in said sample capture pocket.
 27. The method of claim24, wherein a sample of material is discharged to an analyzer selectedfrom the group consisting of a gas chromatograph, a HPLC device, and acombination thereof.